Process of making a superior oil



W. S. BAYLIS PROCESS OF MAKING A SUPERIOR OIL July 12, 1932.

Filed sept. 4. 1928 Con de riser IIIIIIIIIII Prasad J'ulyf 12, 1932 UNITED STATES'- PATENT ori-*lcs man s. Barns, Aor Losv ANGELES, CALIFORNIA, assieme, BY mEsNE AssIGN- HENTS, TO FILTBOL COMPANY F CALIFORNIA, A. CORPORATION OF GALIFORNIA rimessa or MAKING A summon. oIL

' pplication med Septgn'iber .4, 1928. Serial. No. 803,701.

This invention relates to a process by which in the preferred form it is possible to roduce a petroleum lubricatin or transormer oil which has a lower S -gh test, a l better sludging test, and less carbon residue, than any oil which can be produced from similar rawmaterials by any process of which I am aware., If it is not desired to -produce oil of such 1 0 a high grade, I may produce an oil equal to the usual commercial grades of today from a lower grade of raw materials. In case the best gra e of oil is to be made, the starting material is preferably a distilled lubricating `16 stock which may be of thick, thin, lor medium body. In case an ordinary toV very good grade of oil is to be made by my process, I start with what is known as a long residuum, the still bottoms of an oil which has not been distilled down very far. Such material may vary greatly in composition and boilin point accordin to whether a heavy or medium grade of oi is to be produced.

My process requires special apparatus for commercial scale productions, but-it is to be -understood that the apparatus illustrated in the accompanying drawing is not the only one in which the process may be practiced.

Referring to the drawing, the figure shows, 80 in side elevation, and more or less diagrammatically, the preferred apparatus.

In the figure,` 10 is a steam-jacketed agitating tank, capable of withstanding considerable pressure. Its headl 11 accommod-ates two pipes 13 and 14, 13 of large diameter, for introducing a powdered adsorbent, and 14 for 'introducing oil. These pipes are provided with shut-oi valves 13a and 14a reectively. The bottom of the tankvis pro- .K vided with a ve large bottom discharge opening 15. It Ould be twelve inches or more wide. An inlet pipe' 16, of equal width, connects the opening 15 with the top of a reaction chamber 17. In the pipe 16, there is a gate valve 16a.

The reaction chamber is merely a vessel unprovided lwith any agitating gear, but having a large inlet 16 and an equally large outlet 18, having therein a gate valve 18a.

5- More than one reaction chamber may be provided to serve one agitating tank. Heat insulation or a steam jacketmay be provided forthe reaction chamber.

The outlet 18 of the reaction chamber is arranged to `discharge into an extractor 19 of the kind known as the Wilhelm type. Such extractors are described in U. S. latents 1,418,503 and 1,611,095 to Karl l". lVilhelm. 'lhe apparatus shown in either patent may be used. I prefer to use an extractor not more than 13 feet long 6 feet in diameter, and holding not more than 5 tons of an oilclay mixture. f f f r The extractor is provided with a gear or pulley 20 by which its shell-may be rotated about its axle 21. The axle is hollow and accommo'datespiping for a steam inlet 22 and steam outlet 23. The other end forms 'an inlet 24 for a liquid solvent, While 25 is an exit for mixed oil and solvent. 26 is an outlet from the extractor for solvent vapors, leading to a condenser 27. In the pipe 26, there is a dust trap 28. r l

The outlet pipe 29, for mixed oil and sol- Yvent, contains a pump 30 and leads to a still 31, capable of separating accurately, in connection with the condenser 27, the mixture of oil and light solventwhich is distilled in the still 31.

32 is -any suitableV conveying means by which -a dry powder may be conveyed from lthe extractor 19 to a reactivating furnace 33.

The latter. is preferably of the Herresho type, but may be a rotary cylindrical kiln.

From tbe discharge end ofthe kiln, a conveyor 34, capable of handling a powder, is provided. Y

The operation of the process is as follows:

A charge of not more than 21/2 tons of lubricating stock or long residuum is run into the agitating tank 10, and a preferably equally heavycharge of an acid-activated clay is added. The oil may be'preferably slightly acid with HZSO4. The proportion of o il to earth may range from about 20% to 150% by weight, depending on how much of the oil can be absorbed at high temperatures by the adsorbent. The kind of adsorbent Whichl prefer to use is the sulphuric acid-activated clay known commercially as Filtrol.

` While this clay is preferred, on account of j its superior adsorbent qualities, any good ,activated clay ma be used, such as that made according to the United States Patent No. 1,397,113 to P. W. Prutzman. Silica gel is also'suitable.

The mingled oil and clay, which forms a mush or mud, is now heated, by means of the steam jacket, to from 200 F. to 7 50 F., the higher temperatures being used for the more ,viscous and hi her boiling oils. The agitator oil, and this reaction requires time and heat,

it follows that the charge must be kept at a high temperature until this purification is accomplished. The charge is therefore allowed to cool in the reaction chamber forten hours or more; the longer it takes in cooling, the better for the purity of the final product.

This time is of course limited by practical' considerations of output, so'that ten hours may be taken as a practical commercial period although 4a weeks heating would probably cause no inj ur to the oil. The reaction chamber is prefera ly heat insulated to just such an extent that at the end of ten hours the clay will not be greatly (if at all) above the boiling point of the solvent when the latter is added to the clay in the extractor, nor much below that poin When it is desired to discharge the reacted mass into the extractor, the valve v18a is opened, the discharge then taking place by gravity. As soon as this is complete, the valve 18a is again closedand a suitable charge ofa special solvent run into the extractor. It is impossible to prescribe exactly how much solvent is to beused, since the quantity is influenced by the kind of oil desired, the kind of oil under process, and the quality of the adsorbent. In general, however, the amount of solvent should approximate four times the amount of oil processed, by weight.

The kind of solvent used is of extreme importance, since its function is, to be that of being selective in its action. It 'should dissolve the oil retained within the pores of the adsorbent, but it should not extract the color,` ing matter and other colloidal impurities adsorbed on the walls of those pores. `A liquid which performs this function in a very sat isfactory manner is a benzine of Pennsylvania origin which is free from aromatic i compounds and which begins to boil at 140 F. (60 C.) and has its end or dry point at 221 F. (105 (l). This solvent 1s a regularly produced cut of Pennsylvania crude. Other benzines or naphthas of different ori- Tgin will be just as satisfactory if their distillation range is approximately thevsame'and if they are originally free from or have been artificially completely freed from aromatic hydrocarbons.

In the extractor, the oily clay is tumbled with warm solvent until all or nearly all of the oil has been dissolved in the benzine. Ro-

tation is then stopped and after a short settling period the pump 30 is operated, thus l pipe 26 and the dust trap 28 into the condenser 2. Distillation from the still 31 may be practiced at the same time, but the resulting vapors are preferably led to separate condensers. The results of dist-illing are that pure oil is left in the still 31, from which it may be run to storage. If desired, continuous extraction apparatus can be used Without departing from the spirit of the invention.

The residual clay now left in the extractor is Wholly free from solvent and the amount of oil "left in it is small. It is therefore in excellent condition for reactivation.. The chute 32 transfers it to the reactivating furnace 33 in which it is heated to `such a temperature and for such a length of time as to burnout all organic matter andocarbon, but not so highly as-to sinter, glaze, or slag the clay. Persons skilled in the art are capable of performing this step without further directions. 1

The clay is nowin a condition nearly as good as, if not better than, when first used this statement being particularly true vms Filtrol has been used. It is conveyed back I to the agitating tank 10 by the conveyor 34 and may be reused in the process with or without an admixture of fresh clay, moisture and acid. v v

It will be seen, therefore, that I have provided a process in which the benefits of' the thorou h action of a large amount of eicient adsorent ma be realized,"without material -waste of sai adsorbent.

While I have described my process as being applied to mineral oil, I do not limit.

mysel thereto. My invention ma be practiced on vegetable oils, vfor examp e, cottonseed, linseed coconut and soy-bean'oil, animal fats, fish oils, andeven waxes such as parain and ozokerite. In doing so, any aspropriate solvent may be used and full a vantage may be taken -of the known properties of various solvents. The 'test of appro p priateness is whether the solvent will dissolve the desired oil without dissolving the coloring matter and other adsorbed im urities out of the adsorbent. The term o as used in the claims is to'be interpreted broadly enou to cover mineral, animal and vegetable o s, fats and waxes, both crude and refined. l

1 I claim as my invention:

1. In the process of refining oil, Vthe steps which comprise mixing an acid-activated powdered. clay adsorbent with from about to 150% by weight of the oil to be re- 15 fined, heating the mixture to from 200 F. to

750 F., Acooling the mixture from said temeratures in not less than ten hours, extractmg the cooled mass with a solvent capable of removing the oil, but not the coloring matter 2 from the adsorbent, se `arating the oil-laden solution from the soli matter and then recovering the solvent from the oil.

2. A process according to claim 1 in which the solvent is a Pennsylvania benzine.

3. A process according to claim 1 in which the solvent is a benzine free from aromatic hydrocarbons.

4. In the processl of refining oil, the steps which comprise mixing an acid-activated` powdered clay adsorbent .with about 20% to 150% by weight of the oil to be refined, said oil being slig tly acid with H2504, heating the mixture to from 200 F. to 750 F., allow ing the mixture to cool in not less than ten hours, extracting the mixture with a solvent capable of takino-nut the oil but not the col-y orlng matter, ta g out solid matter Jfrom the oil-laden solution and then separating the oil and solvent.

40 5. A process accordin to'claim 4 in which the Lmrened oil is a mineral lubricating Yoil s oc n 6. In a process of refining oil, the steps which comprise mixin an activated mineral fine-pared adsorbent with about 20% to 150% of the oil stock to be refined, heating the mixture to between 200 F. and 750 F., allowing ti mixture to cool in not less than ten hours, and separating the oil from the adsorbent.

In testimony whereof, I have hereunto set my hand at Los Angeles, California, this 22nd day of August, 1928. A

WALTER S.BAYLIS. 

